تفاعل #88421
ord-f7e2c1a181be472c8a441820e6365940
معادلة التفاعل
المتفاعلات
ظروف التفاعل
المعالجة
- 1أخرىobtained in (Example 1.4) <Step 1>
- 2workup.STIRRINGthe obtained mixture was stirred again in a nitrogen atmosphere at 100° C. for 2 hours 40 minutes
- 3استخلاصAn organic layer was extracted
- 4تجفيفwas then dried over anhydrous sodium sulfate
- 5workup.DISTILLATIONThe solvent was distilled away under reduced pressure
- 6أخرىthe obtained residue was then purified by silica gel column chromatography (silica gel:eluent; heptane:ethyl acetate=95:5-50:50)
الإجراء التجريبي
Potassium trifluorovinylborate (172 mg), 1,1′-bis(diphenylphosphino)ferrocene-palladium(II) dichloride (31 mg), and triethylamine (59.4 μl) were added to an ethanol (2.1 ml) solution of the methyl 4-(5-bromo-4-(difluoromethyl)thiazol-2-yl)-1-methyl-1H-pyrazole-5-carboxylate (150 mg) obtained in (Example 1.4) <Step 1>, and the obtained mixture was then stirred in a nitrogen atmosphere at 100° C. for 17 hours. Thereafter, potassium trifluoro(vinyl)borate (342 mg), 1,1′-bis(diphenylphosphino)ferrocene-palladium(II) dichloride (62 mg), and triethylamine (59.4 μl) were added to the reaction solution, and the obtained mixture was stirred again in a nitrogen atmosphere at 100° C. for 2 hours 40 minutes. Thereafter, ethyl acetate (100 ml) and a saturated saline (50 ml) were added to the reaction solution. An organic layer was extracted, and was then dried over anhydrous sodium sulfate. The solvent was distilled away under reduced pressure, and the obtained residue was then purified by silica gel column chromatography (silica gel:eluent; heptane:ethyl acetate=95:5-50:50), so as to obtain the title compound (74 mg) in the form of a colorless solid.